Page 62 - Lab Manual & Project class 12
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LABORATORY MANUAL CHEMISTRY
                                    Oxalate is confirmed by the following tests:

                                    (a)   Acidify sodium carbonate extract with acetic acid and add calcium chloride
                                          solution. A white precipitate of calcium oxalate, insoluble in ammonium
                                          oxalate and oxalic acid solution indicates the presence of oxalate ion.
                                               CaCl  + Na C O  4           CaC O 4         +   2NaCl
                                                          2
                                                    2
                                                                             2
                                                            2
                                                                      Calcium oxalate
                                                                      (White precipitate)
                                    (b)   KMnO  test
                                                4
                                          Filter the precipitate from test (a). Add dil. H SO  to it followed by dilute
                                                                                         4
                                                                                     2
                                          KMnO  solution and warm. Pink colour of KMnO  is discharged:
                                                4
                                                                                           4
                                               CaC O  + H SO                    CaSO          +     H C O
                                                    2  4   2   4                 4            2  2  4
                                   Maxbrain Chemistry
                                                                      Calcium sulphate    Oxalic acid
                                               2 KMnO  + 3H SO  + 5H C O         2MnSO  + K SO  + 8H O + 10CO
                                                       4     2  4     2  2  4           4   2   4    2         2
                                          Pass the gas evolved through lime water. A white precipitate is formed
                                          which dissolves on passing the gas for some more time.

                                 Step-III : Test for Sulphate and Phosphate

                                 If no positive test is obtained in Steps-I and II, then tests for the presence of
                                 sulphate and phosphate ions are performed. These tests are summarised in
                                 Table 7.5.



                                    Table 7.5 : Confirmatory tests for Sulphate and Phosphate

                                 Ion                                 Confirmatory  Test


                         Sulphate ( SO 2–  )       (a)  Take 1 mL water extract of the salt in water or sodium
                                      4                  carbonate  and  after  acidifying  with  dilute
                                                         hydrochloric  acid  add  BaCl solution.  White
                                                                                        2
                                                         precipitate  insoluble  in  conc.  HCl  or  conc.  HNO   is
                                                                                                       3
                                                         obtained.
                                                   (b)  Acidify  the  aqueous  solution  or  sodium  carbonate
                                                         extract with acetic acid and add lead acetate solution.
                                                         Appearance of white precipitate confirms the presence
                                                               2–
                                                         of SO   ion.
                                                               4

                         Phosphate  ( PO 3–  )     (a)  Acidify  sodium  carbonate  extract  or  the  solution  of
                                        4                the salt in water with conc. HNO  and add ammonium
                                                                                       3
                                                         molybdate  solution  and  heat  to  boiling.  A  canary
                                                         yellow  precipitate is  formed.



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